We report the first study dealing with the self-assembly of an α-amino acid derivative in perfluorocarbons. Rheology, microscopy, and spectroscopy studies reveal that the fluorous sodium l-prolinate derivative 1 self-assembles in perfluorocarbons to form a three-dimensional network of left-handed nano-helices resulting in solvent gelation. Singlet oxygen lifetime measured in a gel of perfluorodecalin is about 1000 times longer than in pure water.